EP0847243A1 - Granules coulants a base d'acide organique, procede de production et utilisation - Google Patents

Granules coulants a base d'acide organique, procede de production et utilisation

Info

Publication number
EP0847243A1
EP0847243A1 EP96930104A EP96930104A EP0847243A1 EP 0847243 A1 EP0847243 A1 EP 0847243A1 EP 96930104 A EP96930104 A EP 96930104A EP 96930104 A EP96930104 A EP 96930104A EP 0847243 A1 EP0847243 A1 EP 0847243A1
Authority
EP
European Patent Office
Prior art keywords
acid
granules
organic
granules according
salts
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP96930104A
Other languages
German (de)
English (en)
Inventor
Ulrich Bröckel
Hans Müschen
Joachim Meyer
Beate Salvador
Bruno Käsler
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by BASF SE filed Critical BASF SE
Publication of EP0847243A1 publication Critical patent/EP0847243A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/003—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic followed by coating of the granules
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K30/00—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K30/00—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs
    • A23K30/10—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs of green fodder
    • A23K30/15—Processes specially adapted for preservation of materials in order to produce animal feeding-stuffs of green fodder using chemicals or microorganisms for ensilaging
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K40/00—Shaping or working-up of animal feeding-stuffs
    • A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/30—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using agents to prevent the granules sticking together; Rendering particulate materials free flowing in general, e.g. making them hydrophobic

Definitions

  • the present invention relates to a free-flowing granulate, consisting of a core and a shell, the core material containing an organic acid and a porous carrier and the shell having a water-soluble or water-swellable covering agent.
  • the invention further relates to a process for the production of free-flowing, odor-reduced granules based on organic acids, preferably formic, acetic and / or propionic acid, and the use of the granules for the treatment of food and feed, and for use in silages.
  • organic acids preferably formic, acetic and / or propionic acid
  • liquid organic acids can only be incorporated in concentrated form, for example in animal feed, by considerable technical effort.
  • DE 28 33 727 AI discloses a particulate, fungicidal material which contains propionic acid and a carrier material. With this material, the number of mold colonies in stored agricultural harvest products should not increase even if the incubation period is several days. However, it has been shown that such material itself is not stable in storage (loss of acid) and that the maximum amount of propionic acid which can be applied depends heavily on the carrier material used. In addition, this material gives off unpleasant odors due to the volatilization of the propionic acid.
  • the present invention was therefore based on the object of providing free-flowing, low-odor granules for the treatment of food and animal feed, with which the handling properties for the user are significantly improved.
  • the focus here was on the production of a "solid organic acid" in the form of an adsorbate, which should differ essentially from simple drinking products in that by (a) allowing an acid fraction> 30% by weight in the solid, independent of the carrier material, and thus carrying the highest possible "active ingredient fraction” and (b) limiting the leakage of the organic acid from the adsorbate to a minimum and thus reducing the " Active ingredient content "retained.
  • the powdery end product should have good storage, flow and processing properties.
  • a granulate consisting of a core and a shell, the core material containing an organic acid and a porous carrier and the shell having a cover agent which is water-soluble or water-swellable at 20 ° C.
  • the granulate according to the invention has the advantage that a reduction in the strong pungent acid smell is achieved and the acid component, despite the solid formulation, is readily and quickly released from the solid powder.
  • the invention further relates to a process for the production of granules containing organic acids and porous carrier materials, which is characterized in that the carrier material is soaked with the liquid organic acid, then with a covering agent which is obtained at room temperature stares, is agglomerated, the covering agent being added to such an extent that the resulting granules are coated and, if appropriate, further odorization is carried out by adding fragrances and, if appropriate, the pourability of the agglomerates is ensured by powdering with a finely dispersed powdering agent.
  • Liquid organic acid is understood to mean acids or acid mixtures which are liquid at the processing temperatures or which are converted into liquids by increasing the temperature or dissolving or dispersing them in liquids.
  • the granules according to the invention have a powdering agent on the surface of the casing.
  • the core preferably contains 30-90% by weight, in particular 50-80% by weight, of organic acid.
  • the organic acid preferably consists of one or more Ci-Cg-mono- or di-carboxylic acids, especially formic, acetic and / or propionic acid.
  • Porous, organic or inorganic carrier materials can be used as carriers, the particle sizes of which are between 1 ⁇ m and 1,000 ⁇ m, preferably between 5 ⁇ m and 100 ⁇ m.
  • the core can also contain other solids, for example solids suitable as feed additives, such as Ca propionate.
  • Water-soluble polymers, organic acids, their salts or low-melting inorganic salts can be used as covering agents.
  • Cereal bran, silicates, pearlite or silica are preferably used as carriers in proportions between 10% by weight and 70% by weight, preferably 20 to 40% by weight, based on the weight of the core.
  • Polyethylene glycols, polyvinylpyrrolidones or organic acids and their salts from C3 to C14, preferably C3 to C6, in particular citric acid, fumaric acid, succinic acid, adipic acid, benzoic acid and their salts or amino acids and their salts, are preferably used as covering agents.
  • the carrier material is placed in a mixer, soaked with the organic acid and then agglomerated and coated with the covering agent.
  • the size of the granules can be set by means of process parameters during mixing and also by subsequent sieving or grinding.
  • the granules preferably have an average diameter of less than 3 mm, in particular 0.3-1.3 mm.
  • residual water may be present in the binding liquid used for coating and agglomerating. After the agglomeration process, this water can be bound by a powdering process with a dry and finely dispersed powder. This powdering process also prevents the agglomerates from sticking later and, for example, additionally applies the salt of the organic acid used (for example sodium or calcium propionate) to the agglomerate.
  • a fragrance or flavoring agent is added, such as, for example, vanillin, citral or fructin, as a result of which an additional odor-masking effect and, for example, attracting animal feed intake can be achieved.
  • organic or inorganic porous carriers are suitable for the production of such free-flowing, odor-reduced agglomerates, provided that they are acid-resistant.
  • examples are cereal bran, perlite, clay materials, silicates and silicic acids, preference being given to the inorganic carriers, since their material properties can be better controlled.
  • Particularly suitable covering agents (binding liquids) for the agglomeration process and for coating are those which have a softening temperature of over 30 ° C., preferably over 60 ° C., in order to prevent deformation of the agglomerates at a higher storage temperature. It is preferred to use cover agents which, moreover, do not counteract the pH-lowering action of the adsorbed organic acid or, if appropriate, support or strengthen it.
  • binding liquids For example, highly concentrated, heated sugar solutions or alkali / alkaline earth metal / formate / acetate / propionate solutions are suitable as binding liquids.
  • the final watering step allows their residual water content to be absorbed.
  • Low melting polyethylene glycols such as PEG 4000, melts of citric acid, adipic acid, fumaric acid or benzoic acid or their salts, highly concentrated solutions of amino acids or mixtures of these acids are preferably suitable as binary liquids. 5-80% binding liquid is used, but preferably 10 to 25% by weight, based on the weight of the granulate.
  • suitable powdering agents are themselves finely dispersed, ground organic acids or their salts, for example Na formate, and also inorganic salts or Aerosil. ⁇ 10%, preferably between 0.5 and 5% by weight, of the powdering agents are added.
  • the porous carrier is placed in the mixer, for example, in an Eichrich mixer and soaked with the organic acid at low energy inputs.
  • the procedure can also be such that the liquid is placed in the mixer and the carrier 5 is metered in. In this case, higher energy inputs must be used.
  • the viscosity of the binding liquid should be adjusted by an appropriate temperature selection in such a way that it is below 1,000 mPas, preferably in the range ⁇ 100 mPas, in order to spray the binding fluids.
  • the proportion of these fragrances can be ⁇ 1% by weight, preferably from 0.05 to 0.5% by weight, based on the granules.
  • the agglomerates produced in this way are low in dust, reduce odor and their organic acid content is
  • the granules according to the invention are suitable for the treatment of food and feed, and for use in silages.
  • Food and animal feed are to be understood in particular as crop products such as hay, silage, moist cereals, legumes or cereal fruits, but also milk exchange, liquid, mixed and mineral feed, fish silages or fish meal.
  • the granules according to the invention can also contain other additives, such as minerals, vitamins, antibiotics or protein additives. Examples
  • Sipernat ® roch ⁇ disperse silica, Fa. Degussa
  • an acid mixture consisting of equal parts of formic acid and propionic acid, soaked.
  • the acid mixture is readily absorbed; a loose, free-flowing product is created.
  • the product has a pungent - smelly formic acid / propionic acid smell.
  • Example 2 Analogously to Example 1, 100 g of pearlite are introduced and soaked in formic acid. The acid is readily absorbed, but the product tends to stick and smells strongly of formic acid.
  • Example 2 Analogously to Example 2 were charged with 400 g of Sipernat ® in an Eirich mixer and impregnated with 1.100 g of formic acid; the ants' acidity is then 71%. 260 g of citric acid melt are injected into the mixing chamber at 170 ° C. as a binding liquid from a heated storage container through a two-component nozzle. The resulting agglomerates are powdered with 44 g Sipernat ® and 8 g vanillin. The total acidity is * 74%. The resulting agglomerates are significantly reduced in the smell of formic acid.
  • Powdered Sipernat ® and 24 g vanillin The total acidity is * 74 ..
  • the resulting agglomerates are significantly reduced in smell and easy to pour.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Food Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Zoology (AREA)
  • Organic Chemistry (AREA)
  • Animal Husbandry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Fodder In General (AREA)
  • Fats And Perfumes (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Glanulating (AREA)
  • Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
  • General Preparation And Processing Of Foods (AREA)
  • Detergent Compositions (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Paints Or Removers (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Medicinal Preparation (AREA)
  • Cereal-Derived Products (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

L'invention concerne des granulés coulants composés d'un noyau et d'une enveloppe, qui se caractérisent en ce que le matériau nodal contient un acide organique et un support poreux, l'enveloppe comportant quant à elle un agent de recouvrement soluble ou gonflant dans l'eau à 20 °C.
EP96930104A 1995-08-30 1996-08-26 Granules coulants a base d'acide organique, procede de production et utilisation Withdrawn EP0847243A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19531782A DE19531782A1 (de) 1995-08-30 1995-08-30 Rieselfähiges Granulat auf Basis organischer Säuren, Verfahren zu seiner Herstellung und seine Verwendung
DE19531782 1995-08-30
PCT/EP1996/003757 WO1997007687A1 (fr) 1995-08-30 1996-08-26 Granules coulants a base d'acide organique, procede de production et utilisation

Publications (1)

Publication Number Publication Date
EP0847243A1 true EP0847243A1 (fr) 1998-06-17

Family

ID=7770678

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96930104A Withdrawn EP0847243A1 (fr) 1995-08-30 1996-08-26 Granules coulants a base d'acide organique, procede de production et utilisation

Country Status (19)

Country Link
EP (1) EP0847243A1 (fr)
JP (1) JPH11511969A (fr)
KR (1) KR19990044266A (fr)
CN (1) CN1193892A (fr)
AU (1) AU706207B2 (fr)
BR (1) BR9609990A (fr)
CA (1) CA2227282A1 (fr)
CZ (1) CZ49998A3 (fr)
DE (1) DE19531782A1 (fr)
EA (1) EA000874B1 (fr)
GE (1) GEP20002062B (fr)
HU (1) HUP9802322A3 (fr)
IL (1) IL122355A (fr)
NO (1) NO980861L (fr)
NZ (1) NZ316933A (fr)
PL (1) PL325169A1 (fr)
SK (1) SK22898A3 (fr)
TR (1) TR199800344T1 (fr)
WO (1) WO1997007687A1 (fr)

Families Citing this family (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19710127A1 (de) * 1997-03-12 1998-09-17 Herbert Dr Widulle Mittel zur Keimverminderung im Trinkwasser, Tränkewasser u. Waschwasser für Gemüse
DE19933906A1 (de) * 1999-07-22 2001-01-25 Eckhard Eltz Verfahren und Anordnung zur Behandlung von Futtermitteln
DE10055390A1 (de) * 2000-11-09 2002-05-29 Nutrinova Gmbh Einsatz eines Säurepräparates als Futtermittelzusatz in der Nutztieraufzucht
BR0306806A (pt) * 2002-01-08 2004-12-07 Can Technologies Inc Ingrediente de alimentação encapsulado
KR100451545B1 (ko) * 2002-03-18 2004-10-06 김유용 염산과 규산염광물질을 함유한 자돈사료첨가용 혼합조성물의 제조방법, 상기 혼합조성물 및 사료
DE10231891A1 (de) * 2002-07-12 2004-01-22 Basf Ag Zubereitungen, enthaltend Diformiate
SE528410C2 (sv) * 2004-06-30 2006-11-07 Kemira Grow How Ab Antimikrobiell surgörande foderprodukt och förfarande för dess framställning
WO2006082240A1 (fr) * 2005-02-04 2006-08-10 Basf Aktiengesellschaft Materiau gonflant dans l’eau
DE102006021392B4 (de) * 2006-05-08 2013-06-27 Ligrana Gmbh Zusammensetzung
DE102007031039A1 (de) * 2007-07-04 2009-01-08 Süd-Chemie AG Verfahren zur schonenden Raffination von Pflanzenölen mit Naturbleicherde
LU500270B1 (en) 2021-06-10 2022-12-12 Lucas Brendler Carboxylic Acid Loaded Salt Carrier and the Method for Producing thereof
DE102021115047A1 (de) 2021-06-10 2022-12-15 André Brendler Carbonsäure beladener Salzträger und das Verfahren zur Herstellung davon

Family Cites Families (13)

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Publication number Priority date Publication date Assignee Title
NL149989B (nl) * 1967-03-08 1976-07-15 Philips Nv Korrelvormig preparaat.
CH484625A (de) * 1969-04-03 1970-01-31 Libavia Ag Verfahren zur Herstellung granulierter Futtermittel
AR206283A1 (es) * 1971-01-27 1976-07-15 Chinoin Gyogyszer Es Vegyeszet Una composicion para la conservacion de productos de procedencia animal o vegetal
CH613607A5 (en) * 1975-06-11 1979-10-15 Lonza Ag Ensiling agent and process for preparation thereof
US4199606A (en) * 1977-09-22 1980-04-22 Bland Bobby Propionic acid on a carrier material as a preservative
DE3103623A1 (de) * 1979-08-03 1982-09-16 Siegfried Dr. 8069 Sünzhausen Moser "mineralstoffreiches ergaenzungsfutter und dessen verwendung"
IT1185550B (it) * 1985-04-12 1987-11-12 Dox Al Italia Spa Miscele non polverose di sfarinati o farine con principi attivi per mangimistica
IT1229930B (it) * 1988-10-14 1991-09-16 Dox Al Italia Spa Procedimento per la preparazione di miscele per uso alimentare e mangimistico comprendenti sostanze attive distribuite in modo uniforme
US5082675A (en) * 1989-07-29 1992-01-21 Bp Chemicals Limited Ensiling composition
DE4117399A1 (de) * 1990-06-14 1992-01-09 Micro Plus Konzentrate Gmbh Wasserhaltiges mittel zur konditionierung feinkoerniger mineralischer futtermittel
DE4217971C1 (de) * 1992-05-30 1993-10-21 Boehringer Ingelheim Vetmed Verfahren und Wirbelbettapparatur zum Granulieren und/oder Umhüllen
EP0612843A1 (fr) * 1993-02-22 1994-08-31 Unilever N.V. Agents de nettoyage acides granulaires
IT1265290B1 (it) * 1993-12-17 1996-10-31 Dox Al Italia Spa Miscele ad elevato contenuto di sostanze attive idonee ad essere distribuite in modo omogeneo nei mangimi per animali.

Non-Patent Citations (1)

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Title
See references of WO9707687A1 *

Also Published As

Publication number Publication date
MX9801399A (es) 1998-05-31
HUP9802322A2 (hu) 1999-01-28
CN1193892A (zh) 1998-09-23
WO1997007687A1 (fr) 1997-03-06
TR199800344T1 (xx) 1998-05-21
AU6928696A (en) 1997-03-19
PL325169A1 (en) 1998-07-06
AU706207B2 (en) 1999-06-10
CA2227282A1 (fr) 1997-03-06
NO980861D0 (no) 1998-02-27
SK22898A3 (en) 1998-12-02
EA199800229A1 (ru) 1998-12-24
HUP9802322A3 (en) 2001-08-28
IL122355A0 (en) 1998-04-05
BR9609990A (pt) 1999-07-06
NZ316933A (en) 1999-01-28
CZ49998A3 (cs) 1998-08-12
DE19531782A1 (de) 1997-03-06
JPH11511969A (ja) 1999-10-19
GEP20002062B (en) 2000-05-10
IL122355A (en) 2000-08-31
NO980861L (no) 1998-02-27
EA000874B1 (ru) 2000-06-26
KR19990044266A (ko) 1999-06-25

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